CN110436429A - A kind of method that thermal decomposition method prepares battery-grade iron phosphate - Google Patents
A kind of method that thermal decomposition method prepares battery-grade iron phosphate Download PDFInfo
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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Abstract
The present invention discloses a kind of method that thermal decomposition method prepares battery-grade iron phosphate.Iron powder is reacted with the mixing of phosphoric acid urea solution, it is 50-65 DEG C of reaction 2-3h in temperature that the molar ratio of iron powder and urea phosphate, which is 1:1.005-1.01, and the pH reacted to terminal is 3.5-4.5, then stops reaction, and filtering obtains filter residue and filtrate；By filtrate by being spray-dried, spray drying material is obtained, spray-drying process inlet air temperature is 250-300 DEG C, and drop temperature≤60 DEG C obtain spray drying material；Spray drying material is calcined in rotary kiln, calcination temperature is 450-600 DEG C, calcination time 3-5h, and cooling discharging, vacuum packaging obtains battery-grade iron phosphate.Present invention process is simple, at low cost, and no waste water generates, obtained ferric phosphate large specific surface area, and activity is high, is suitble to prepare the LiFePO4 of high capacity, low temperature performance well.
Description
Technical field
The present invention relates to a kind of methods that thermal decomposition method prepares battery-grade iron phosphate, belong to lithium battery new energy materials neck
Domain.
Background technique
Ferric phosphate also known as high ferric phosphate,Ferric orthophosphate, molecular formula FePO4, it is a kind of white, canescence monoclinic crystal
Powder.It is the material of white slightly powder containing the crystallization water, anhydrous iron phosphate is the slightly yellow material of white.Its main application is to make
Make lithium iron phosphate cell material, catalyst and ceramics etc..
LiFePO4 is prepared at present, it is presoma that most of producer, which is all made of battery-grade anhydrous iron phosphate, conventional at present
The preparation process of battery-grade anhydrous iron phosphate is as follows: ferrous salt and phosphate, oxidant hybrid reaction are obtained containing the crystallization water
Ferric phosphate obtain the ferric phosphate dried feed containing the crystallization water by washing, dry, by high-temperature calcination obtain LITHIUM BATTERY without
Water ferric phosphate.
But this technique has the following problems:
1, waste water yield is very big, due to needing to wash away anion and other cations, so product per ton needs are several
Ten tons to up to a hundred tons of washes；
2, long flow path is needed by ingredient, reaction, washing, drying, calcining and other processes.
3, process control is more difficult, needs each index of controlled reaction-precipitation object, and the production cycle is long, general entire work
Sequence needs at least 30 are more than hour.
4, at high cost, production efficiency is low, needs artificial more.
Summary of the invention
In view of this, the present invention provides a kind of method that thermal decomposition method prepares battery-grade iron phosphate, simple process, cost
Low, no waste water generates, obtained ferric phosphate large specific surface area, and activity is high, is suitble to prepare the ferric phosphate of high capacity, low temperature performance well
Lithium.
The present invention solves above-mentioned technical problem by following technological means:
A kind of method that thermal decomposition method prepares battery-grade iron phosphate, is following steps: iron powder and phosphoric acid urea solution is mixed
Conjunction is stirred to react, and the molar ratio of iron powder and urea phosphate is 1:1.005-1.01, is 50-65 DEG C of reaction 2-3h in temperature, reaction is extremely
The pH of terminal is 3.5-4.5, then stops reaction, and filtering obtains filter residue and filtrate；
By filtrate by being spray-dried, spray drying material is obtained, spray-drying process inlet air temperature is 250-300 DEG C, out
Material temperature degree≤60 DEG C obtain spray drying material；
Spray drying material is calcined in rotary kiln, calcination temperature is 450-600 DEG C, calcination time 3-5h, calcined
Journey is passed through air and maintains oxygen quality score >=18% in the atmosphere in rotary furnace, cooling discharging, and vacuum packaging obtains battery
Grade ferric phosphate.
The purity of the iron powder is greater than 99.0%, Ni/Co≤30ppm, Zn/Cd/Pb≤20ppm, Mn≤100ppm, Ca/
Mg/Na/K≤50ppm。
The concentration of the phosphoric acid urea solution is 1.8-2.5mol/L, Ni/Co≤15mg/L, Zn/Cd/Pb in phosphoric acid urea solution
≤ 25mg/L, Mn≤50mg/L, Ca/Mg/Na/K≤40mg/L.
Mixing speed when being stirred to react is 100-150r/min, and obtained filter residue return continues after mixing with iron powder
Reaction is reacted after the simple substance iron content into filter residue is lower than 100ppm and is abandoned.
Spray-drying process makes the size controlling of droplet to 10-50 μm, residence time of the droplet in spray dryer
For 5-15S, the partial size for being spray-dried material is 3-10 μm, is spray-dried the water content of material lower than 1%.
The steam obtained when spray drying returns to dissolving phosphoric acid urea by the pure water that condensing recovery obtains after filtering and obtains
To phosphoric acid urea solution.
In rotary furnace calcination process, the revolving speed of rotary kiln is 2-4r/min, and calcination process opens air-introduced machine, in rotary kiln
Gas flow rate be 3-6m/S, be passed through 100-200 times that volume of air in rotary kiln is rotary kiln volume, rotary kiln per hour
The big 50-100Pa of pressure in the interior pressure ratio external world, rotary kiln drop temperature≤60 DEG C.
Iron is removed using air-flow crushing and electromagnetism before vacuum packaging, being crushed to material particular diameter is 1-3 μm.
So this technique does not generate waste water, returns and use after condensation in the vapor that spray drying obtains, Ke Yishi
Existing water recycles, and simple process only allows iron powder to react with urea phosphate in the stage of reaction, obtains soluble salt, then
Then again in rotary kiln, by high-temperature calcination, while sky is passed through by spray drying so as to form the crystallization of molysite urea phosphate
Gas oxidation, obtains ferric phosphate, other organic matters are calcination into carbon dioxide and vapor at high temperature, big so as to obtain
The battery-grade iron phosphate of surface area.It, can be with so as to prevent growing up for ferric phosphate primary particle size due to the generation of bulk gas
Obtain the battery-grade anhydrous iron phosphate that primary particle size is less than 100nm.
This patent process is short, is divided into three dissolution, spray drying and calcining steps, so that production efficiency is substantially increased,
Also save manpower.
Cost is relatively low for this patent, and according to calculating, the cost of ferric phosphate per ton is lower than 9000 yuan.
The beneficial effects of the present invention are: simple process and low cost, no waste water is generated, obtained ferric phosphate large specific surface area,
It is active high, it is suitble to prepare the LiFePO4 of high capacity, low temperature performance well.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in detail, and a kind of thermal decomposition method of the present embodiment prepares electricity
The method of pond grade ferric phosphate, is following steps: iron powder and phosphoric acid urea solution being mixed and reacted, and iron powder and urea phosphate rub
You are 50-65 DEG C of reaction 2-3h in temperature than being 1:1.005-1.01, and the pH reacted to terminal is 3.5-4.5, are then stopped anti-
It answers, filters, obtain filter residue and filtrate；
By filtrate by being spray-dried, spray drying material is obtained, spray-drying process inlet air temperature is 250-300 DEG C, out
Material temperature degree≤60 DEG C obtain spray drying material；
Spray drying material is calcined in rotary kiln, calcination temperature is 450-600 DEG C, calcination time 3-5h, calcined
Journey is passed through air and maintains oxygen quality score >=18% in the atmosphere in rotary furnace, cooling discharging, and vacuum packaging obtains battery
Grade ferric phosphate.
The purity of the iron powder is greater than 99.0%, Ni/Co≤30ppm, Zn/Cd/Pb≤20ppm, Mn≤100ppm, Ca/
Mg/Na/K≤50ppm。
The concentration of the phosphoric acid urea solution is 1.8-2.5mol/L, Ni/Co≤15mg/L, Zn/Cd/Pb in phosphoric acid urea solution
≤ 25mg/L, Mn≤50mg/L, Ca/Mg/Na/K≤40mg/L.
Mixing speed when being stirred to react is 100-150r/min, and obtained filter residue return continues after mixing with iron powder
Reaction is reacted after the simple substance iron content into filter residue is lower than 100ppm and is abandoned.
Spray-drying process makes the size controlling of droplet to 10-50 μm, residence time of the droplet in spray dryer
For 5-15S, the partial size for being spray-dried material is 3-10 μm, is spray-dried the water content of material lower than 1%.
The steam obtained when spray drying returns to dissolving phosphoric acid urea by the pure water that condensing recovery obtains after filtering and obtains
To phosphoric acid urea solution.
In rotary furnace calcination process, the revolving speed of rotary kiln is 2-4r/min, and calcination process opens air-introduced machine, in rotary kiln
Gas flow rate be 3-6m/S, be passed through 100-200 times that volume of air in rotary kiln is rotary kiln volume, rotary kiln per hour
The big 50-100Pa of pressure in the interior pressure ratio external world, rotary kiln drop temperature≤60 DEG C.
Iron is removed using air-flow crushing and electromagnetism before vacuum packaging, being crushed to material particular diameter is 1-3 μm.
Embodiment 1
A kind of method that thermal decomposition method prepares battery-grade iron phosphate, is following steps: iron powder and phosphoric acid urea solution is mixed
Conjunction is stirred to react, and the molar ratio of iron powder and urea phosphate is 1:1.008, is 62 DEG C of reaction 2.5h in temperature, is reacted pH to terminal
It is 3.9, then stops reaction, filtering obtains filter residue and filtrate；
By filtrate by being spray-dried, spray drying material is obtained, spray-drying process inlet air temperature is 280 DEG C, out material temperature
≤ 60 DEG C of degree obtains spray drying material；
Spray drying material is calcined in rotary kiln, calcination temperature is 550 DEG C, calcination time 4.2h, and calcination process is logical
Enter air and maintain oxygen quality score >=18% in the atmosphere in rotary furnace, cooling discharging, vacuum packaging obtains LITHIUM BATTERY phosphorus
Sour iron.
It is as a result as follows by iron powder sample detection:
Phosphoric acid urea solution is prepared, testing result is as follows:
| Index | Concentration | Ni | Co | Zn | Cd | Pb |
| Numerical value | 1.9mol/L | 1.5ppm | 2.1ppm | 6.4ppm | 0.2ppm | 0.1ppm |
| Mn | Ca | Mg | Na | K | Fe | Cu |
| 4.7ppm | 12.5ppm | 14.2ppm | 10.4ppm | 2.1ppm | 2.1ppm | 0.1ppm |
Mixing speed when being stirred to react is 130r/min, and continuation is instead after obtained filter residue return mix with iron powder
It answers, reacts after the simple substance iron content into filter residue is lower than 100ppm and abandon.
Spray-drying process makes the size controlling of droplet to 10-50 μm, residence time of the droplet in spray dryer
For 12S, the partial size for being spray-dried material is 6.8 μm, is spray-dried the water content of material lower than 1%.
The steam obtained when spray drying returns to dissolving phosphoric acid urea by the pure water that condensing recovery obtains after filtering and obtains
To phosphoric acid urea solution.
In rotary furnace calcination process, the revolving speed of rotary kiln is 3r/min, and calcination process opens air-introduced machine, in rotary kiln
Gas flow rate is 4.5m/S, and the volume of air being passed through in rotary kiln per hour is 160 times of rotary kiln volume, the pressure in rotary kiln
Power is 70Pa bigger than extraneous pressure, rotary kiln drop temperature≤60 DEG C.
Iron is removed using air-flow crushing and electromagnetism before vacuum packaging, being crushed to material particular diameter is 2.1 μm.
Finally obtained anhydrous iron phosphate product testing result is as follows:
| Index | Iron phosphorus ratio | High temperature moisture | D10 | D50 | D90 |
| Numerical value | 0.991 | 0.098% | 1.01μm | 2.1μm | 4.76μm |
| D100 | Cd | Co | Pb | Ca | Na |
| 6.12μm | 3.4ppm | 10.1ppm | 0.9ppm | 21.5ppm | 4.9ppm |
| Ni | Mn | Zn | Cr | Al | Ti |
| 19.8ppm | 26.8ppm | 6.1ppm | 12.1ppm | 2.1ppm | 1.1ppm |
| Tap density | Sulphur | Chloride ion | BET | Magnetic foreign body | |
| 0.65g/mL | 10.1ppm | 2.1ppm | 21.6m2/g | 0.98ppm |
Embodiment 2
A kind of method that thermal decomposition method prepares battery-grade iron phosphate, is following steps: iron powder and phosphoric acid urea solution is mixed
Conjunction is stirred to react, and the molar ratio of iron powder and urea phosphate is 1:1.008, is 60 DEG C of reaction 2.5h in temperature, is reacted pH to terminal
It is 4.2, then stops reaction, filtering obtains filter residue and filtrate；
By filtrate by being spray-dried, spray drying material is obtained, spray-drying process inlet air temperature is 290 DEG C, out material temperature
≤ 60 DEG C of degree obtains spray drying material；
Spray drying material is calcined in rotary kiln, calcination temperature is 550 DEG C, calcination time 4.5h, and calcination process is logical
Enter air and maintain oxygen quality score >=18% in the atmosphere in rotary furnace, cooling discharging, vacuum packaging obtains LITHIUM BATTERY phosphorus
Sour iron.
The purity of the iron powder is greater than 99.0%, Ni/Co≤30ppm, Zn/Cd/Pb≤20ppm, Mn≤100ppm, Ca/
Mg/Na/K≤50ppm。
The concentration of the phosphoric acid urea solution is 2.2mol/L, Ni/Co≤15mg/L in phosphoric acid urea solution, Zn/Cd/Pb≤
25mg/L, Mn≤50mg/L, Ca/Mg/Na/K≤40mg/L.
Mixing speed when being stirred to react is 140r/min, and continuation is instead after obtained filter residue return mix with iron powder
It answers, reacts after the simple substance iron content into filter residue is lower than 100ppm and abandon.
Spray-drying process makes the size controlling of droplet to 10-50 μm, residence time of the droplet in spray dryer
For 12S, the partial size for being spray-dried material is 7.4 μm, is spray-dried the water content of material lower than 1%.
The steam obtained when spray drying returns to dissolving phosphoric acid urea by the pure water that condensing recovery obtains after filtering and obtains
To phosphoric acid urea solution.
In rotary furnace calcination process, the revolving speed of rotary kiln is 3.2r/min, and calcination process opens air-introduced machine, in rotary kiln
Gas flow rate be 5.5m/S, 180 times that volume of air in rotary kiln is rotary kiln volume are passed through per hour, in rotary kiln
The big 85Pa of pressure in the pressure ratio external world, rotary kiln drop temperature≤60 DEG C.
Iron is removed using air-flow crushing and electromagnetism before vacuum packaging, being crushed to material particular diameter is 1.9 μm.
Finally obtained product testing result is as follows:
| Index | Iron phosphorus ratio | High temperature moisture | D10 | D50 | D90 |
| Numerical value | 0.989 | 0.102% | 0.93μm | 1.9μm | 3.88μm |
| D100 | Cd | Co | Pb | Ca | Na |
| 4.32μm | 3.9ppm | 12.1ppm | 0.4ppm | 23.6ppm | 5.8ppm |
| Ni | Mn | Zn | Cr | Al | Ti |
| 12.8ppm | 23.2ppm | 6.6ppm | 11.1ppm | 2.4ppm | 1.4ppm |
| Tap density | Sulphur | Chloride ion | BET | Magnetic foreign body | |
| 0.61g/mL | 15.6ppm | 1.5ppm | 25.7m2/g | 0.99ppm |
Embodiment 3
A kind of method that thermal decomposition method prepares battery-grade iron phosphate, is following steps: iron powder and phosphoric acid urea solution is mixed
Conjunction is stirred to react, and the molar ratio of iron powder and urea phosphate is 1:1.009, is 61 DEG C of reaction 2.6h in temperature, is reacted pH to terminal
It is 4.4, then stops reaction, filtering obtains filter residue and filtrate；
By filtrate by being spray-dried, spray drying material is obtained, spray-drying process inlet air temperature is 265 DEG C, out material temperature
≤ 60 DEG C of degree obtains spray drying material；
Spray drying material is calcined in rotary kiln, calcination temperature is 550 DEG C, and calcination time 4h, calcination process is passed through
Air simultaneously maintains oxygen quality score >=18% in atmosphere in rotary furnace, and cooling discharging, vacuum packaging obtains LITHIUM BATTERY phosphoric acid
Iron.
The purity of the iron powder is greater than 99.0%, Ni/Co≤30ppm, Zn/Cd/Pb≤20ppm, Mn≤100ppm, Ca/
Mg/Na/K≤50ppm。
The concentration of the phosphoric acid urea solution is 1.95mol/L, Ni/Co≤15mg/L in phosphoric acid urea solution, Zn/Cd/Pb≤
25mg/L, Mn≤50mg/L, Ca/Mg/Na/K≤40mg/L.
Mixing speed when being stirred to react is 130r/min, and continuation is instead after obtained filter residue return mix with iron powder
It answers, reacts after the simple substance iron content into filter residue is lower than 100ppm and abandon.
Spray-drying process makes the size controlling of droplet to 10-50 μm, residence time of the droplet in spray dryer
For 15S, the partial size for being spray-dried material is 9.5 μm, is spray-dried the water content of material lower than 1%.
The steam obtained when spray drying returns to dissolving phosphoric acid urea by the pure water that condensing recovery obtains after filtering and obtains
To phosphoric acid urea solution.
In rotary furnace calcination process, the revolving speed of rotary kiln is 3.5r/min, and calcination process opens air-introduced machine, in rotary kiln
Gas flow rate be 5.5m/S, 140 times that volume of air in rotary kiln is rotary kiln volume are passed through per hour, in rotary kiln
The big 95Pa of pressure in the pressure ratio external world, rotary kiln drop temperature≤60 DEG C.
Iron is removed using air-flow crushing and electromagnetism before vacuum packaging, being crushed to material particular diameter is 2.5 μm.
| Index | Iron phosphorus ratio | High temperature moisture | D10 | D50 | D90 |
| Numerical value | 0.992 | 0.115% | 1.25μm | 2.5μm | 4.12μm |
| D100 | Cd | Co | Pb | Ca | Na |
| 4.65μm | 5.1ppm | 10.3ppm | 0.8ppm | 20.4ppm | 5.1ppm |
| Ni | Mn | Zn | Cr | Al | Ti |
| 11.4ppm | 29.7ppm | 6.1ppm | 11.9ppm | 2.1ppm | 1.1ppm |
| Tap density | Sulphur | Chloride ion | BET | Magnetic foreign body | |
| 0.69g/mL | 18.4ppm | 1.1ppm | 22.7m2/g | 0.91ppm |
The anhydrous iron phosphate that the anhydrous iron phosphate that embodiment 1,2 and 3 obtains is obtained with liquid phase synthesis on the market is using phase
LiFePO4 is prepared with technique, final result is as follows:
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (8)
1. a kind of method that thermal decomposition method prepares battery-grade iron phosphate, which is characterized in that be following steps: by iron powder and urea phosphate
Solution, which is mixed, to react, and the molar ratio of iron powder and urea phosphate is 1:1.005-1.01, is 50-65 DEG C of reaction 2-3h in temperature,
The pH of reaction to terminal is 3.5-4.5, then stops reaction, and filtering obtains filter residue and filtrate；
By filtrate by being spray-dried, spray drying material is obtained, spray-drying process inlet air temperature is 250-300 DEG C, out material temperature
≤ 60 DEG C of degree obtains spray drying material；
Spray drying material is calcined in rotary kiln, calcination temperature is 450-600 DEG C, calcination time 3-5h, and calcination process is logical
Enter air and maintain oxygen quality score >=18% in the atmosphere in rotary furnace, cooling discharging, vacuum packaging obtains LITHIUM BATTERY phosphorus
Sour iron.
2. the method that a kind of thermal decomposition method according to claim 1 prepares battery-grade iron phosphate, it is characterised in that: the iron
The purity of powder is greater than 99.0%, Ni/Co≤30ppm, Zn/Cd/Pb≤20ppm, Mn≤100ppm, Ca/Mg/Na/K≤50ppm.
3. the method that a kind of thermal decomposition method according to claim 1 prepares battery-grade iron phosphate, it is characterised in that: the phosphorus
The concentration of sour urea solution is 1.8-2.5mol/L, Ni/Co≤15mg/L in phosphoric acid urea solution, Zn/Cd/Pb≤25mg/L, Mn≤
50mg/L, Ca/Mg/Na/K≤40mg/L.
4. the method that a kind of thermal decomposition method according to claim 1 prepares battery-grade iron phosphate, it is characterised in that: described to stir
Mixing mixing speed when reaction is 100-150r/min, and the reaction was continued after obtained filter residue return is mixed with iron powder, reaction to filter
Simple substance iron content in slag is abandoned after being lower than 100ppm.
5. the method that a kind of thermal decomposition method according to claim 1 prepares battery-grade iron phosphate, it is characterised in that: spraying dry
Dry process makes the size controlling of droplet to 10-50 μm, and residence time of the droplet in spray dryer is 5-15S, spraying dry
The partial size of dry material is 3-10 μm, is spray-dried the water content of material lower than 1%.
6. the method that a kind of thermal decomposition method according to claim 1 prepares battery-grade iron phosphate, it is characterised in that: spraying dry
The steam obtained when dry returns to dissolving phosphoric acid urea by the pure water that condensing recovery obtains after filtering and obtains phosphoric acid urea solution.
7. the method that a kind of thermal decomposition method according to claim 1 prepares battery-grade iron phosphate, it is characterised in that: turning round
In furnace calcination process, the revolving speed of rotary kiln is 2-4r/min, and calcination process opens air-introduced machine, and the gas flow rate in rotary kiln is 3-
6m/S, the volume of air being passed through in rotary kiln per hour are 100-200 times of rotary kiln volume, and the pressure ratio in rotary kiln is extraneous
The big 50-100Pa of pressure, rotary kiln drop temperature≤60 DEG C.
8. the method that a kind of thermal decomposition method according to claim 1 prepares battery-grade iron phosphate, it is characterised in that: vacuum packet
Iron is removed using air-flow crushing and electromagnetism before dress, being crushed to material particular diameter is 1-3 μm.
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| CN111232944A (en) * | 2020-03-19 | 2020-06-05 | 王敏 | Preparation method of low-cost iron phosphate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708834A (en) * | 2009-12-11 | 2010-05-19 | 广西壮族自治区化工研究院 | Wafer-like ferric phosphate, preparation method and application thereof |
| CN102491302A (en) * | 2011-12-15 | 2012-06-13 | 湖北万润新能源科技发展有限公司 | Battery-grade anhydrous iron phosphate and preparation method thereof |
| CN102745662A (en) * | 2012-06-15 | 2012-10-24 | 兰州理工大学 | Preparation method of amorphous iron phosphate |
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- 2019-09-11 CN CN201910858979.9A patent/CN110436429B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101708834A (en) * | 2009-12-11 | 2010-05-19 | 广西壮族自治区化工研究院 | Wafer-like ferric phosphate, preparation method and application thereof |
| CN102491302A (en) * | 2011-12-15 | 2012-06-13 | 湖北万润新能源科技发展有限公司 | Battery-grade anhydrous iron phosphate and preparation method thereof |
| CN102745662A (en) * | 2012-06-15 | 2012-10-24 | 兰州理工大学 | Preparation method of amorphous iron phosphate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111232944A (en) * | 2020-03-19 | 2020-06-05 | 王敏 | Preparation method of low-cost iron phosphate |
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Effective date of registration: 20210918 Address after: 618200 Xinshi Industrial Development Zone, Mianzhu City, Deyang City, Sichuan Province (zone a) Patentee after: SICHUAN LOMON PHOSPHOROUS CHEMISTRY Co.,Ltd. Address before: 317399 No.9, building 53, Nanmen new village, Xianju County, Taizhou City, Zhejiang Province Patentee before: Li Xuyi |